固体酸S2O8^2-/Nb2O5/La^3+的制备、表征及催化合成乙酸正丁酯  

Preparation and Characterization of Solid Acid S2O8^2-/Nb2O5/La^3+ Catalyst and Its Catalytic Performance in Synthesis of n-Butyl Acetate

作　　者：徐常龙[1] 曹小华[1] 曹良林 陈慧 吴从锦 罗宇进 XU Chang-long;CAO Xiao-hua;CAO Liang-lin;CHEN Hui;WU Cong-jin;LUO Yu-jin(College of Chemical and Environmental Engineering,Jiujiang University,Jiujiang 332005,China)

机构地区：[1]九江学院化学与环境工程学院,江西九江332005

出　　处：《合成化学》2020年第11期983-988,共6页Chinese Journal of Synthetic Chemistry

基　　金：国家自然科学基金资助项目(21864015);江西省教育厅科技项目(GJJ180892);2019年国家级大学生创新创业训练计划(201911843018)。

摘　　要：以Nb2O5为载体,浸渍法研制固体酸(S2O8^2-/Nb2O5/La+)催化剂,经SEM、XRD和EDS表征,考察了固体酸的焙烧温度、陈化时间及S2O8^2-浓度等因素对该催化剂催化活性的影响。结果表明:在(NH4)2S2O8浓度为1 mol/L、浸渍时间18 h、w(La^3+)=3%(基于Nb2O5的质量)、焙烧温度为500℃时,制备出最高催化效果的催化剂。接着考察了其催化合成乙酸正丁酯的催化活性,通过正交实验确定了反应的最佳条件:n(正丁醇)/n(冰醋酸)=2.0/1.0、催化剂用量w(S2O8^2-/Nb2O5/La^3+)=2.9%、反应温度为125℃,反应时间为3.0 h,酯化率为95.7%。催化剂循环利用3次后仍有90.1%的酯化率。The Solid acid catalyst S2O8^2-/Nb2O5/La^3+was prepared by impregnation method with niobium oxide as carrier and was characterized through SEM,XRD and EDS.The effects of catalyst calcination temperature,aging time and S2O8^2- concentration on the catalytic activity of the catalyst were investigated.The experimental results show that the optimized of catalyst preparation recipe includes impregnation concentration of 1 mol/L ammonium persulfate,the amount of La^3+was 3.0%of the mass of total Nb2O5,impregnation time 18 h,calcination temperature of 500℃.The optimum conditions of the esterification reaction were as follows:mole ratio of n-butanol to acetic acid(2/1),the mass of catalyst 2.9%based on the total raw materials,reaction temperature 125℃and reaction time 3.0 h.Under above conditions,the yield of n-butyl acetate could reach 95.7%.Esterification rate could retain 90.1%after the catalyst being used 3 times.

关 键 词：固体酸S2O8^2-/Nb2O5/La^+ 氧化铌 催化 乙酸正丁酯 制备 

分 类 号：TQ426.6[化学工程] O62[理学—有机化学]